CN103011125B - Method of preparing mesoporous carbon material and application of mesoporous carbon material as noble metal catalyst carrier - Google Patents
Method of preparing mesoporous carbon material and application of mesoporous carbon material as noble metal catalyst carrier Download PDFInfo
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Abstract
The invention provides a method of preparing a mesoporous carbon material. The method comprises the steps of: based on soybean as a raw material, conducting grinding and ball milling, and carrying out thermal treatment and carbonization under the protection of inert gas to prepare mesoporous carbon; washing mesoporous carbon with acetone, filtering to remove residues in carbonization process, drying and treating with mixed water solution of nitric acid and hydrogen peroxide, and oxidizing, cleaning, filtering and drying the surfaces of mesoporous carbon; then conducting thermal treatment and secondary carbonization under the protection of inert gas; and finally conducting atmospheric oxidization treatment to the secondarily-carbonized material with the mixed water solution of nitric acid and hydrogen peroxide, filtering and washing to be neutral, and drying to obtain the mesoporous carbon material. The mesoporous carbon material prepared is large in specific area and high in activity; and when the mesoporous carbon material is used for noble metal catalyst carriers, the effective utilization ratio of the catalyst can be greatly improved, and the usage amount of noble metal and the cost of catalyst can be reduced.
Description
Technical field
The present invention relates to a kind of preparation method of meso-porous carbon material, relate in particular to a kind of method of utilizing soya bean to prepare meso-porous carbon material; The present invention also relates to the application of this meso-porous carbon material as precious metal catalyst agent carrier simultaneously.
Background technology
Fuel battery energy is directly converted into electric energy by the chemical energy in fuel and oxygenant, and without burning, therefore transformation efficiency can be up to 60% ~ 80%, is considered to the ultimate form of human use's energy.But fuel cell is also in industrialization eve at present, its major cause is that the cost of the catalyzer (Pt Base Metal and alloy thereof) that is applied to fuel cell is high, and catalyst activity is not high, and resistance to corrosion also needs the problems such as further raising.Therefore, the emphasis of fuel cell studies should be development catalyst technology, reduce costs at present, breaks through the application bottleneck of fuel cell.
Carbon support is one of critical material of fuel-cell catalyst, and it not only directly affects dispersity and the catalytic activity of catalyzer, and the load transfer in Catalytic Layer and mass transfer process are also had to material impact.In fuel-cell catalyst, carbon support is had to following requirement: 1, high conductivity: to reduce electrode internal resistance; 2, high-specific surface area: be conducive to dispersed activity component, reduce noble metal dosage; 3, rational pore structure and hydrophobic nature: meet the mass transfer requirement of gas and reaction product; 4, the interaction between carbon support and active ingredient: improve catalytic activity; 5, in fuel cell operation environment, there is good chemical stability and thermostability.Therefore the development of fuel-cell catalyst carrier, has very important impact to the performance of fuel cell, selects to have bigger serface, and the carrier that active group or atom are contained in surface, can improve the catalytic activity of catalyzer, reduce the loss of catalyzer, increase the life-span of catalyzer.
Meso-porous carbon material has the features such as pore volume stores high, surperficial condensing characteristic good, thermostability and chemical stability is high, conductive capability is strong, therefore, seems pratical and feasible as fuel-cell catalyst carrier.
Summary of the invention
The object of this invention is to provide a kind of preparation method of meso-porous carbon material.
Another object of the present invention is to provide this meso-porous carbon material support of the catalyst in the application of preparing in fuel cell.
The preparation method of meso-porous carbon material of the present invention, a kind of preparation method of meso-porous carbon material, is take soya bean as raw material, after pulverizing, ball milling, under protection of inert gas, in 600 ~ 1000 ℃ of charing 1 ~ 2 h, makes mesoporous carbon; Then mesoporous carbon is cleaned with acetone after ball milling 2 ~ 4 h in ball mill, filter the residue of removing in carbonization process, dry; Process 12 ~ 24 h with the mixed aqueous solution of nitric acid and hydrogen peroxide in stirring at room temperature again, make mesoporous carbon surface oxidation, after cleaning, filter, being dried, under protection of inert gas, in 600 ~ 1000 ℃ of secondary charing 1 ~ 2 h; The finally mixed aqueous solution with nitric acid and hydrogen peroxide by secondary char-forming material, oxide treatment 12 ~ 24 h under room temperature, washing, to neutral, is filtered, and is dried and obtains.
It is that the mesoporous carbon after ball milling is fully distributed in acetone that described acetone cleans, and 1 ~ 2 h refluxes at 50 ~ 60 ℃; The consumption of acetone is 10 ~ 30 ml/g.
In the mixed aqueous solution of described nitric acid and hydrogen peroxide, the concentration of nitric acid is 1 ~ 2 molL
-1, H
2o
2 mass percent 1 ~ 10%.The consumption of the mixed aqueous solution of nitric acid and hydrogen peroxide is 10 ~ 30 mlg.
Described being dried is in convection oven, in 40 ~ 80 ℃ of dry 12 ~ 24h.
Fig. 1 is rear meso-porous carbon material N after a charing of the present invention
2-adsorption desorption graphic representation (adopting full-automatic specific surface area and lacunarity analysis instrument, Kang Ta company of the U.S.).Show after tested, after a charing of the present invention, the specific surface area of meso-porous carbon material is 176 m
2g
-1.
Fig. 2 be after a charing of invention the graph of pore diameter distribution of meso-porous carbon material (according to N
2-desorption curve negotiating BJH algorithm calculates).Show after tested, after a charing of the present invention, the pore size of meso-porous carbon material is 3.7 nm, and even aperture distribution.
Fig. 3 is the N of meso-porous carbon material after secondary charing of the present invention
2-Adsorption and desorption isotherms figure (adopting full-automatic specific surface area and lacunarity analysis instrument, Kang Ta company of the U.S.).Show after tested, after secondary charing of the present invention, the BET test pattern of meso-porous carbon material is typical IV type adsorption curve, illustrates that the carbon material obtaining is meso-porous carbon material, and specific surface has reached 517 m
2g
-1, and the specific surface area of most widely used carrier VulcanXC-72R carbon black is 233 m
2g
-1, show that this meso-porous carbon material has larger specific surface area, has more the advantage as support of the catalyst.
Fig. 4 is that the graph of pore diameter distribution of meso-porous carbon material after secondary charing of the present invention is (according to N
2-desorption curve negotiating BJH algorithm calculates).Show after tested, after secondary charing of the present invention, the pore size of meso-porous carbon material is 3.7 nm, and even aperture distribution, and the load that is more conducive to metal contacts with micromolecular with catalyzer.
Fig. 5 is the X ray electron-diffraction diagram (XRD) after the meso-porous carbon material carried noble metal Pt for preparing of the present invention.Can be clearly seen that (111), (200), (220), (311) and (222) crystal face of Pt Pt/Soybean and Pt/C from Fig. 5, in Pt/C the crystal face diffraction peak of Pt a little less than, in Pt/Soybean, the crystal face diffraction peak of Pt is stronger, illustrates that the Pt metal face-centered cubic form being out reduced exists.
Fig. 6 be after the carbon material supported precious metal of New Type of Mesoporous 20 % wt Pt/Soybean and Pt/C at H
2sO
4cO stripping figure in solution, that calculates known CO stripping peak plays that spike potential is negative has moved 12.4mV, shows to have better anti-CO poisoning capability after meso-porous carbon material loaded metal, by the calculating to CO stripping peak area, EAS
cO-Pt/Soybean=57.16m
2g
-1, EAS
cO-Pt/C=45.94 m
2g
-1, show that Pt/Soybean specific activity Pt/C is active large.
Fig. 7 be after the meso-porous carbon material carried noble metal prepared of the present invention 20%wt Pt/Soybean and Pt/C at 0.5 M CH
3oH/H
2sO
4cyclic voltammetry figure in solution.Result shows, the peak current of Pt/Soybean catalyst methyl alcohol is 1.5 times of peak current of Pt/C catalyst methyl alcohol, plays that spike potential is negative has moved 50 mV, and the catalytic activity of surperficial Pt/Soybean catalyzer is better than Pt/C catalyzer.
Fig. 8 is at saturated N after New Type of Mesoporous carbon material supported precious metal 20wt% Pt/Soybean and Pt/C
20.5 M CH
3oH+0.5 M H
2sO
4chronoamperogram in solution, significantly sees that the good stability of Pt/Soybean catalyzer is in Pt/C catalyst stability.
In sum, the relative prior art of meso-porous carbon material of the present invention has the following advantages:
1, meso-porous carbon material of the present invention is take analysis for soybean powder as raw material, makes carbonization process more thorough through twice carbonization, the load of the more suitable catalyzer in aperture and micromolecular entering; After processing by acetone, hydrogen peroxide and acid, make its surface obtain functionalization, can play the fixed action to micromolecular absorption and catalyzer, can effectively solve that the activity of conventional carbon carrier in fuel-cell catalyst is low, specific surface area is little, the problems such as catalyst activity particle easily comes off, increase substantially the effective rate of utilization of catalyzer, reduce the usage quantity of precious metal and the cost of catalyzer.
2, material soya bean of the present invention is biological environmental production recyclable materials, can be used for scale operation and industrialization.
3, the meso-porous carbon material that prepared by the present invention reaches 517 m through twice charing specific surface area
2g
-1, promoted the transmission of reaction intermediate, thereby the interface that catalyzed reaction is occurred obtains expansion, has accelerated catalytic process, makes full use of the catalytic active site of Pt, therefore this carrier is a kind of more satisfactory Pt base and alloy as catalyst agent carrier thereof.
Accompanying drawing explanation
Fig. 1 is the N of meso-porous carbon material after a charing
2-adsorption desorption graphic representation;
Fig. 2 is aperture-pore volume distribution plan of meso-porous carbon material after a charing;
Fig. 3 is meso-porous carbon material N after secondary charing
2-adsorption desorption Curve chart;
Fig. 4 is aperture-pore volume distribution plan of meso-porous carbon material after secondary charing;
Fig. 5 is the XRD figure of 20%wt Pt/Soybean and Pt/C;
Fig. 6 is that 20%wt Pt/Soybean and Pt/C are at saturated N
20.5M H
2sO
4cO stripping figure in solution;
Fig. 7 is that 20%wt Pt/Soybean and Pt/C are at 0.5 M CH
3oH/H
2sO
4cyclic voltammetry figure in solution;
Fig. 8 is that 20%wt Pt/Soybean and Pt/C are at saturated N
20.5 M CH
3oH+0.5 M H
2sO
4chronoamperogram in solution;
Embodiment
The preparation of the preparation below by specific embodiment to meso-porous carbon material of the present invention and supporting Pt base and alloy catalyst thereof is described further.
(1) preparation of meso-porous carbon material
By after soya bean pulverizing, ball milling refinement, in protection of inert gas, 800 ℃ of charing 2 h, make mesoporous carbon; By mesoporous carbon ball milling 4 h.Take the mesoporous carbon after 2 g ball millings, join in the acetone of 30 ml, in to 60 ℃ of 2 h that reflux, clean, remove by filter the residue in carbonization process; Be placed in convection oven in 60 ℃ of dry 12 h.Join that in the nitric acid of 30 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 2 mol/L, H
2o
2mass percent be 3%), stirring at normal temperature is processed 24 h, makes mesoporous carbon surface oxidation; After cleaning, filtering in convection oven 60 ℃ of dry 12 h.Then mesoporous carbon surface cleaning being oxidized is again in protection of inert gas, and secondary charing 2h at 800 ℃, makes its carbonization more complete; Finally join that in the nitric acid of 30 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 2 mol/L, H
2o
2mass percent be 3%), Oxidation at room temperature is processed 24 h, suction filtration, deionized water rinsing, to neutral, then, at 60 ℃ of dry 12 h of blast dry oven, obtain meso-porous carbon material Soybean, productive rate is 9.0%.
(2) preparation of Pt/Soybean catalyzer: add 30 ml EG, 15 ml deionized waters in 250 ml round-bottomed flasks, then add 33.0 mg Potassium Hydrogen Phthalates, ultrasonic agitation is to dissolving completely; Add 100 mg meso-porous carbon material Soybean to stir; Adding 66.4 mg Platinic chlorides to stir dissolves it completely; With pH value=10 of ethylene glycol solution (content of KOH the is 5%) regulator solution of KOH, then after ultrasonic 40 min; Add (ethylene glycol 60 ml, water 30 ml, sodium borohydride 80 mg) in the ethylene glycol of sodium borohydride and the solution of water reaction 2 h; Filter, be neutral with deionized water repetitive scrubbing to filtrate, in vacuum drying oven, 60 ℃ of dry 12 h, obtain platinum catalyst.
In platinum catalyst, the mass ratio of Pt and meso-porous carbon material is 1:4; The electric current that Pt/Soybean catalyzer produces is 1.5 times of Pt/C catalyzer.
(1) preparation of meso-porous carbon material
By after soya bean pulverizing, ball milling refinement, in protection of inert gas, 900 ℃ of charing 1 .5h, make mesoporous carbon; By mesoporous carbon ball milling 4 h in ball mill.Take the mesoporous carbon after 2 g ball millings, join in the acetone of 25 ml, in 60 ℃ of 2 h that reflux, clean, remove by filter the residue in carbonization process; Be placed in convection oven, at 60 ℃ of dry 12 h; Then join that in the nitric acid of 25 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1 mol/L, H
2o
2mass percent be 5%), stirring at normal temperature is processed 24 h, makes mesoporous carbon surface oxidation; Cleaning, filtration are placed in convection oven, at 50 ℃ of dry 12 h.Then in protection of inert gas, secondary charing 1.5h at 900 ℃, makes its carbonization more complete; Finally join that in the nitric acid of 25 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1 mol/L, H
2o
2mass percent be 5%), Oxidation at room temperature is processed 24 h, suction filtration, deionized water rinsing, to neutral, after filtration, at 60 ℃ of dry 12 h of blast dry oven, obtain meso-porous carbon material Soybean, productive rate is 8.3%.
(2) preparation of PtRuIr/Soybean catalyzer: in 250 ml round-bottomed flasks, add 30 ml EG, 15 ml deionized waters and 33.0 mg Potassium Hydrogen Phthalates, ultrasonic agitation is to dissolving completely; Add again 100 mg meso-porous carbon material Soybean to stir, then add 38.2 mg Platinic chlorides, 9.87 mg ruthenium trichlorides, 19.0 mg nickelous chlorides, continue stirring it is dissolved completely; With pH value=10 of ethylene glycol solution (KOH content the is 5%) regulator solution of KOH, then, after ultrasonic 40 min, dropwise drip (ethylene glycol 60 ml, water 30 ml, sodium borohydride 80 mg) in the ethylene glycol of sodium borohydride and the solution of water reaction 2 h; Filter, and be neutral with deionized water repetitive scrubbing to filtrate, in vacuum drying oven, 60 ℃ of dry 12 h, obtain PtRuIr/Soybean catalyzer.In catalyzer, the mass ratio of PtRuIr and meso-porous carbon material is 1:4, wherein Pt:Ru:Ir=2:1:1.
The electric current that PtRuIr/Soybean catalyzer produces is 1.2 times of PtRuIr/C catalyzer.
embodiment 3
(1) preparation of meso-porous carbon material
By after soya bean pulverizing, ball milling refinement, in protection of inert gas, 1000 ℃ of charing 1 h, make mesoporous carbon, with ball mill ball milling 4 h.Take 2 g mesoporous carbon and join in the acetone of 20 ml, in 55 ℃ of 2 h that reflux, clean, remove by filter after the residue in carbonization process, be placed in convection oven, at 60 ℃ of dry 12h.Then add that in the nitric acid of 20 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1 mol/L, H
2o
2mass percent be 10%), stirring at room temperature is processed 12 h, makes mesoporous carbon surface oxidation; After cleaning, filtering, in convection oven, 50 ℃ are dried 12 h; In protection of inert gas, 1000 ℃ of secondary charing 2 h, make its carbonization more complete again; Product joins that in the nitric acid of 20 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1mol/L, H
2o
2mass percent be 10%), Oxidation at room temperature is processed 24 h, deionized water rinsing, to neutral, after filtration, at 60 ℃ of dry 12 h of blast dry oven, obtains meso-porous carbon material Soybean, productive rate is 7.8%.
(2) preparation of PtNi/Soybean catalyzer: in 250 ml round-bottomed flasks, add 30 ml EG, 15 ml deionized waters and 33.0 mg Potassium Hydrogen Phthalates, ultrasonic agitation is to dissolving completely; Add again 100 mg meso-porous carbon materials to stir; Then adding 53.3 mg Platinic chlorides, 13.2 mg nickelous chlorides to stir dissolves it completely; With pH value=10 of ethylene glycol solution (content of KOH the is 5%) regulator solution of KOH, after ultrasonic 40 min, dropwise drip (ethylene glycol 60 ml, water 30 ml, sodium borohydride 80 mg) reaction 2 h in the ethylene glycol of sodium borohydride and the solution of water; Suction filtration, is neutral with deionized water repetitive scrubbing to filtrate, and in vacuum drying oven, 60 ℃ of dry 12 h, obtain PtNi/Soybean catalyzer.In catalyzer, the mass ratio of PtNi and meso-porous carbon material is 1:4, wherein Pt:Ni=4:1.
The electric current of PtNi/Soybean catalyzer improves 20% compared with PtNi/C catalyzer.
(1) preparation of meso-porous carbon material
By after soya bean pulverizing, ball milling refinement, in protection of inert gas, 700 ℃ of mesoporous carbon that charing next time makes, with ball mill ball milling 4 h.Take the mesoporous carbon after 2 g ball millings, join in the acetone of 50 ml, in 60 ℃ of 2 h that reflux, clean, remove by filter after the residue in carbonization process, be placed in convection oven, at 60 ℃ of dry 12 h; Join that in the nitric acid of 50ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1.5 mol/L, H
2o
2mass percent be 8%), stirring at room temperature is processed 12 h, makes mesoporous carbon surface oxidation; Washing, filter after in convection oven 60 ℃ of dry 12 h; Again in protection of inert gas, 700 ℃ of charing 2 h again, make its carbonization more complete; Finally join that in the nitric acid of 50 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 1.5 mol/L, H
2o
2mass percent be 8%), Oxidation at room temperature is processed 12h, suction filtration is neutral with deionized water rinsing to filtrate, at 60 ℃ of dry 12 h of blast dry oven, obtains meso-porous carbon material Soybean, productive rate is 8.9%.
(2) preparation of PtRu/Soybean catalyzer: in 250 ml round-bottomed flasks, add 30 mLEG, 15 mL deionized waters and 33.0 mg Potassium Hydrogen Phthalates, ultrasonic agitation is to dissolving completely; Add again 100 mg meso-porous carbon materials to stir; Then adding 43.7 mg Platinic chlorides, 22.6 mg ruthenium trichlorides to stir dissolves it completely, with pH value=10 of ethylene glycol solution (KOH content the is 5%) regulator solution of KOH, after ultrasonic 40 min, dropwise drip (ethylene glycol 60 ml in the ethylene glycol of sodium borohydride and the solution of water, water 30 ml, sodium borohydride 80 mg), reaction 2 h; Filtering, is neutral with deionized water repetitive scrubbing to filtrate, and in vacuum drying oven, 60 ℃ of dry 12 h, obtain PtRu/Soybean catalyzer.In catalyzer, the mass ratio of PtRu and meso-porous carbon material is 1:4, wherein Pt:Ru=1:1(atomic ratio).
The electric current of PtRu/Soybean catalyzer improves 35% compared with PtRu/C catalyzer.
embodiment 5
(1) preparation of meso-porous carbon material
By after soya bean pulverizing, ball milling refinement, in protection of inert gas, 600 ℃ of mesoporous carbon that charing makes, with ball mill ball milling 4 h.Take 2 g mesoporous carbon and join in the acetone of 60 ml, in 60 ℃ of 2 h that reflux, clean, remove by filter after the residue in carbonization process, be placed in 40 ℃ of dry 24 h in convection oven.Join that in the nitric acid and hydrogen peroxide mixed aqueous solution of 60 ml, (concentration of nitric acid is 2 mol/L, H
2o
2mass percent be 1%), stirring at room temperature is processed 24 h, makes mesoporous carbon surface oxidation; Washing, filter after in convection oven 40 ℃ of dry 24h; In protection of inert gas, 600 ℃ of secondary charing 2h, make its carbonization more complete again; Finally join that in the nitric acid of 60 ml and the mixed aqueous solution of hydrogen peroxide, (concentration of nitric acid is 2 mol/L, H
2o
2mass percent be 1%), Oxidation at room temperature is processed 24 h, deionized water rinsing, suction filtration to filtrate is neutral, at 40 ℃ of dry 24h of blast dry oven, obtains meso-porous carbon material Soybean, productive rate is 9.4%.
(2) preparation of PtRu/Soybean catalyzer: in 250 ml round-bottomed flasks, add 30 ml EG, 15 ml deionized waters, 33.0 mg Potassium Hydrogen Phthalates, ultrasonic agitation is to dissolving completely; Add again 100 mg meso-porous carbon materials to stir; Then add 56.6 mg Platinic chlorides, 9.7 mg ruthenium trichlorides, stir it is dissolved completely; With pH value=10 of ethylene glycol solution (content of KOH the is 5%) regulator solution of KOH, after ultrasonic 40 min, dropwise drip (ethylene glycol 60 ml, water 30 ml, sodium borohydride 80 mg) in the ethylene glycol of sodium borohydride and the solution of water reaction 2h; Filter, be neutral with deionized water repetitive scrubbing to filtrate, 60 ℃ of dry 12h in vacuum drying oven, obtain PtRu/C catalyzer.In catalyzer, the mass ratio of PtRu and meso-porous carbon material is 1:4, wherein Pt:Ru=3:1.
The electric current of PtRu/Soybean catalyzer improves 10% compared with PtRu/C catalyzer.
Claims (4)
1. a preparation method for meso-porous carbon material, is take soya bean as raw material, after pulverizing, ball milling, under protection of inert gas, in 600
1000 ℃ of charings 1
2 h, make mesoporous carbon; Then by mesoporous carbon ball milling 2 in ball mill
after 4 h, clean with acetone, filter the residue of removing in carbonization process, dry; Process 12 with the mixed aqueous solution of nitric acid and hydrogen peroxide in stirring at room temperature again
24 h, make mesoporous carbon surface oxidation, after cleaning, filter, being dried, under protection of inert gas, in 600
1000 ℃ of secondary charings 1
2 h; The finally mixed aqueous solution with nitric acid and hydrogen peroxide by secondary char-forming material, oxide treatment 12 under room temperature
24 h, washing, to neutral, is filtered, dry and obtain.
2. the preparation method of meso-porous carbon material as claimed in claim 1, is characterized in that: it is that the mesoporous carbon after ball milling is fully distributed in acetone, in 50 that described acetone cleans
at 60 ℃, reflux 1
2 h.
3. the preparation method of meso-porous carbon material as claimed in claim 1, is characterized in that: described dry be in convection oven, in 40
80 ℃ dry 12
24h.
4. the preparation method of meso-porous carbon material as claimed in claim 1, is characterized in that: in the mixed aqueous solution of described nitric acid and hydrogen peroxide, the concentration of nitric acid is 1
2 molL
-1, H
2o
2mass percent 1
10%.
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| CN106410229B (en) * | 2016-10-14 | 2020-09-15 | 三峡大学 | Preparation method and application of supported carbon-based fuel cell anode catalyst |
| CN110649272A (en) * | 2019-09-29 | 2020-01-03 | 先进储能材料国家工程研究中心有限责任公司 | Preparation process of catalyst for proton exchange membrane fuel cell |
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